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Modeling the X-ray Process, and X-ray Flaw Size Parameter for POD Studies

Nondestructive evaluation (NDE) method reliability can be determined by a statistical flaw detection study called probability of detection (POD) study. In many instances, the NDE flaw detectability is given as a flaw size such as crack length. The flaw is either a crack or behaving like a crack in terms of affecting the structural integrity of the material. An alternate approach is to use a more complex flaw size parameter. The X-ray flaw size parameter, given here, takes into account many setup and geometric factors. The flaw size parameter relates to X-ray image contrast and is intended to have a monotonic correlation with the POD. Some factors such as set-up parameters, including X-ray energy, exposure, detector sensitivity, and material type that are not accounted for in the flaw size parameter may be accounted for in the technique calibration and controlled to meet certain quality requirements. The proposed flaw size parameter and the computer application described here give an alternate approach to conduct the POD studies. Results of the POD study can be applied to reliably detect small flaws through better assessment of effect of interaction between various geometric parameters on the flaw detectability. Moreover, a contrast simulation algorithm for a simple part-source-detector geometry using calibration data is also provided for the POD estimation.

Koshti, Ajay M.↗

Non-Destructive Evaluation of Materials via Ultraviolet Spectroscopy

A document discusses the use of ultraviolet spectroscopy and imaging for the non-destructive evaluation of the degree of cure, aging, and other properties of resin-based composite materials. This method can be used in air, and is portable for field use. This method operates in reflectance, absorbance, and luminescence modes. The ultraviolet source is used to illuminate a composite surface of interest. In reflectance mode, the reflected response is acquired via the imaging system or via the spectrometer. The spectra are analyzed for organic compounds (conjugated organics) and inorganic compounds (semiconducting band-edge states; luminescing defect states such as silicates, used as adhesives for composite aerospace applications; and metal oxides commonly used as thermal coating paints on a wide range of spacecraft). The spectra are compared with a database for variation in conjugation, substitution, or length of molecule (in the case of organics) or band edge position (in the case of inorganics). This approach is useful in the understanding of material quality. It lacks the precision in defining the exact chemical structure that is found in other materials analysis techniques, but it is advantageous over methods such as nuclear magnetic resonance, infrared spectroscopy, and chromatography in that it can be used in the field to assess significant changes in chemical structure that may be linked to concerns associated with weaknesses or variations in structural integrity, without disassembly of or destruction to the structure of interest.

Pugel, Betsy↗

Advanced X-Ray Inspection of Reinforced Carbon Composite Materials on the Orbiter Leading Edge Structural Subsystem (LESS)

The post return-to-flight (RTF) inspection methodology for the Orbiter Leading Edge Structural Subsystem (LESS) is currently being defined. Numerous NDT modalities and techniques are being explored to perform the flight-to-flight inspections of the reinforced carbon/carbon (RCC) composite material for impact damage, general loss of mass in the bulk layers, or other anomalous conditions that would pose risk to safe return upon re-entry. It is possible to have an impact upon ascent that is not visually observable on the surface, yet causes internal damage. Radiographic testing may be a useful NDT technique for such occurrences. The authors have performed radiographic tests on full-sized mock samples of LESS hardware with embedded image quality phantoms. Digitized radiographic film, computed radiography and flat panel digital real-time radiography was acquired using a GE Eresco 200 x-ray tube, and Se-75 and Yb-169 radioisotopes.

Hernandez, Jose M.↗

Structural Anomalies Detected in Ceramic Matrix Composites Using Combined Nondestructive Evaluation and Finite Element Analysis (NDE and FEA)

Most reverse engineering approaches involve imaging or digitizing an object and then creating a computerized reconstruction that can be integrated, in three dimensions, into a particular design environment. The rapid prototyping technique builds high-quality physical prototypes directly from computer-aided design files. This fundamental technique for interpreting and interacting with large data sets is being used here via Velocity2 (an integrated image-processing software, ref. 1) using computed tomography (CT) data to produce a prototype three-dimensional test specimen model for analyses. A study at the NASA Glenn Research Center proposes to use these capabilities to conduct a combined nondestructive evaluation (NDE) and finite element analysis (FEA) to screen pretest and posttest structural anomalies in structural components. A tensile specimen made of silicon nitrite (Si3N4) ceramic matrix composite was considered to evaluate structural durability and deformity. Ceramic matrix composites are being sought as candidate materials to replace nickel-base superalloys for turbine engine applications. They have the unique characteristics of being able to withstand higher operating temperatures and harsh combustion environments. In addition, their low densities relative to metals help reduce component mass (ref. 2). Detailed three-dimensional volume rendering of the tensile test specimen was successfully carried out with Velocity2 (ref. 1) using two-dimensional images that were generated via computed tomography. Subsequent, three-dimensional finite element analyses were performed, and the results obtained were compared with those predicted by NDE-based calculations and experimental tests. It was shown that Velocity2 software can be used to render a three-dimensional object from a series of CT scan images with a minimum level of complexity. The analytical results (ref. 3) show that the high-stress regions correlated well with the damage sites identified by the CT scans and the experimental data. Furthermore, modeling of the voids collected via NDE offered an analytical advantage that resulted in more accurate assessments of the material s structural strength. The top figure shows a CT scan image of the specimen test section illustrating various hidden structural entities in the material and an optical image of the test specimen considered in this study. The bottom figure represents the stress response predicted from the finite element analyses (ref .3 ) for a selected CT slice where it clearly illustrates the correspondence of the high stress risers due to voids in the material with those predicted by the NDE. This study is continuing, and efforts are concentrated on improving the modeling capabilities to imitate the structural anomalies as detected.

Abdul-Aziz, Ali↗

Bond Line Thickness Estimation in Composite Structures Using Multiple Inspection Techniques

Imaging and other nondestructive evaluation techniques are commonly used for material characterization and defect recognition in safety critical aerospace applications, with data fusion providing the framework for uncertainty quantification in these contexts. Most commonly, forward physics-based modeling predicts the response conditioned on material properties and defect assumptions, and probabilistic methods are used to infer the hidden state of the subject of the inspection from a combination of prior information, likelihoods, and inspection data. In this paper Bayesian methods are used to estimate bond thickness in lap joints comprised of aluminum adherends using a combination of infrared thermography and ultrasound. The concept of the conflation of probability distributions is applied to combine the posterior distributions derived from thermography and ultrasound and the quality of the fused estimates are compared against the individual estimates against synthetic data that was created to mimic the inspection of a lap joint comprised of aluminum adherends.

thermal nondestructive evaluation↗

NASA Tech Briefs, September 2008

Topics covered include: Nanotip Carpets as Antireflection Surfaces; Nano-Engineered Catalysts for Direct Methanol Fuel Cells; Capillography of Mats of Nanofibers; Directed Growth of Carbon Nanotubes Across Gaps; High-Voltage, Asymmetric-Waveform Generator; Magic-T Junction Using Microstrip/Slotline Transitions; On-Wafer Measurement of a Silicon-Based CMOS VCO at 324 GHz; Group-III Nitride Field Emitters; HEMT Amplifiers and Equipment for their On-Wafer Testing; Thermal Spray Formation of Polymer Coatings; Improved Gas Filling and Sealing of an HC-PCF; Making More-Complex Molecules Using Superthermal Atom/Molecule Collisions; Nematic Cells for Digital Light Deflection; Improved Silica Aerogel Composite Materials; Microgravity, Mesh-Crawling Legged Robots; Advanced Active-Magnetic-Bearing Thrust- Measurement System; Thermally Actuated Hydraulic Pumps; A New, Highly Improved Two-Cycle Engine; Flexible Structural-Health-Monitoring Sheets; Alignment Pins for Assembling and Disassembling Structures; Purifying Nucleic Acids from Samples of Extremely Low Biomass; Adjustable-Viewing-Angle Endoscopic Tool for Skull Base and Brain Surgery; UV-Resistant Non-Spore-Forming Bacteria From Spacecraft-Assembly Facilities; Hard-X-Ray/Soft-Gamma-Ray Imaging Sensor Assembly for Astronomy; Simplified Modeling of Oxidation of Hydrocarbons; Near-Field Spectroscopy with Nanoparticles Deposited by AFM; Light Collimator and Monitor for a Spectroradiometer; Hyperspectral Fluorescence and Reflectance Imaging Instrument; Improving the Optical Quality Factor of the WGM Resonator; Ultra-Stable Beacon Source for Laboratory Testing of Optical Tracking; Transmissive Diffractive Optical Element Solar Concentrators; Delaying Trains of Short Light Pulses in WGM Resonators; Toward Better Modeling of Supercritical Turbulent Mixing; JPEG 2000 Encoding with Perceptual Distortion Control; Intelligent Integrated Health Management for a System of Systems; Delay Banking for Managing Air Traffic; and Spline-Based Smoothing of Airfoil Curvatures.

Source record↗

Study Thermographic Flaw Detection

The development of thermographic inspection methods for use on aerospace structures is under investigation. Several different material systems, structural geometries and defect types have been included in this study so as to establish a baseline from which future IRT testing can be made. This study examines various thermal loading techniques in an attempt to enhance the likelihood of capturing and identifying critically sized flaws under 'non-laboratory' actual working conditions. Qualification techniques and calibration standards are also being investigated to standardize the thermographic method. In conjunction with the thermographic inspections, advanced image processing techniques including digital filtering and neural networks have been investigated to increase the ability of 91 detecting and sizing flaws. Here, the digitized thermographic images are mathematically manipulated through various filtering techniques and/or artificial neural mapping schemes to enhance its overall quality, permitting accurate flaw identification even when the signal-to-noise ratio is low.

Walker, James L.↗

Study Thermographic Flaw Detection

The development of thermographic inspection methods for use on aerospace structures is under investigation. Several different material systems, structural geometries and defect types have been included in this study so as to establish a baseline from which future Infrared Thermography(IRT) testing can be made. This study examines various thermal loading techniques in an attempt to enhance the likelihood of capturing and identifying critically sized flaws under 'non laboratory' actual working conditions. Qualification techniques and calibration standards are also being investigated to standardize the thermographic method. In conjunction with the thermographic inspections, advanced image processing techniques including digital filtering and neural networks have been investigated to increase the ability of detecting and sizing flaws. Here, the digitized thermographic images are mathematically manipulated through various filtering techniques and/or artificial neural mapping schemes to enhance its overall quality, permitting accurate flaw identification even when the signal-to-noise ratio is low.

Walker, James L.↗

The importance of properties in modeling

Casting and welding of superalloys, stainless steel and titanium alloys are processes which can be improved through modeling of heat flow, fluid flow, residual stress development, and microstructural evolution. These simulations require inputs of thermophysical data, some of which involves the partially or totally liquid state. In particular, these processes involve melting, flow in the liquid, and solidification. Modeling of such processes can lead to an improved understanding of defects such as shrinkage, inclusions, cracks, incomplete filling (or penetration), macrosegregation, improper grain structure, and deviations from dimensional specifications. Effective modeling can shorten process development time and improve quality. An approach to these problems is to develop efficient models; validate through correlations with thermal, distortion, and microstructural data; run parametric studies; extract knowledge based rules; and apply to adaptive closed loop control systems. With the appropriate pre- and post-processing, such analyses can be made 'user friendly'. This would include graphical user interfaces as well as realistic images and color maps. In such form, these models can be used for sensitivity analyses, which are useful in defining appropriate sensors and in the development of control strategies. Such modeling can be done at several levels, e.g., the MARO level, modeling large scale phenomena such as heat and fluid flow or material deformation; the MICRO level, modeling the development of dendrites, grains or precipitates; or at the NANO level, modeling point defects, dislocations, stacking faults, etc. There are many computational issues associated with these simulations, e.g. computational efficiency and accuracy. In addition, there are many materials issues, not the least of which is the availability of accurate high temperature thermophysical data for complex alloys. This would include latent heat of fusion, temperature dependent heat capacity and thermal conductivity (for liquid and solid), viscosity, surface tension, thermal expansion, mechanical properties, etc. Preliminary data is frequently gathered from the literature; however, this is often not available for modern alloys. If additional data are required, measurements can be used; however, these are costly, time consuming and can be erroneous due to a lack of testing standards or impure materials. Microstructural predictors can be extracted from thermal information, e.g. cooling rate and thermal gradient; the prediction of microstructure is dependent on solidus and liquidus temperature, mushy zone permeability, the solidification curve, volume changes, phase transformations, alloying effects (such as surface tension or viscosity), mold/metal reactions, metal/environment reactions, etc. Defect maps may be needed to predict the onset of shrinkage, hot cracking or 'freckling'. Constants may be needed for stress relaxation, dendrite coarsening, vaporization, etc. Visualization was used as a tool to better comprehend complex data sets associated with the analysis of directional solidification (including crystal growth) and welding. Examples include not only isotherms, but also cooling rate, growth rate and thermal gradient. The latter two are not single valued scalars, but rather time and space dependent vector fields. Efficient models were developed for both casting and welding to predict heat flow and the relationship to dendrite and grain growth. These codes include many of the non-linear effects, e.g. radiation, which dominate these processes. The home-built FDM code(s) were designed to be useful not only to the scientist, but also to the process engineer. Special output can be requested to compare directly to experimental data. Visualization procedures were developed to visualize critical results, e.g. fusion zone width at the surface opposite that where the arc is applied ('penetration'). Both elaborate and simplified distortion analyses were carried out. It is clear that extensive mechanical property data are critical in order to accurately predict residual stress patterns. A scheme is currently being developed to integrate these modeling tools into a set of control algorithms; however, the success of this approach is critically dependent on the availability of accurate high temperature thermophysical data.

Giamei, A. F.↗

Fluorescent Approaches to High Throughput Crystallography

We have shown that by covalently modifying a subpopulation, less than or equal to 1%, of a macromolecule with a fluorescent probe, the labeled material will add to a growing crystal as a microheterogeneous growth unit. Labeling procedures can be readily incorporated into the final stages of purification, and the presence of the probe at low concentrations does not affect the X-ray data quality or the crystallization behavior. The presence of the trace fluorescent label gives a number of advantages when used with high throughput crystallizations. The covalently attached probe will concentrate in the crystal relative to the solution, and under fluorescent illumination crystals show up as bright objects against a dark background. Non-protein structures, such as salt crystals, will not incorporate the probe and will not show up under fluorescent illumination. Brightly fluorescent crystals are readily found against less bright precipitated phases, which under white light illumination may obscure the crystals. Automated image analysis to find crystals should be greatly facilitated, without having to first define crystallization drop boundaries as the protein or protein structures is all that shows up. Fluorescence intensity is a faster search parameter, whether visually or by automated methods, than looking for crystalline features. We are now testing the use of high fluorescence intensity regions, in the absence of clear crystalline features or "hits", as a means for determining potential lead conditions. A working hypothesis is that kinetics leading to non-structured phases may overwhelm and trap more slowly formed ordered assemblies, which subsequently show up as regions of brighter fluorescence intensity. Preliminary experiments with test proteins have resulted in the extraction of a number of crystallization conditions from screening outcomes based solely on the presence of bright fluorescent regions. Subsequent experiments will test this approach using a wider range of proteins. The trace fluorescently labeled crystals will also emit with sufficient intensity to aid in the automation of crystal alignment using relatively low cost optics, further increasing throughput at synchrotrons.

Pusey, Marc L.↗

NIAC Phase I Study Final Report on Large Ultra-Lightweight Photonic Muscle Space Structures

The research goal is to develop new tools support NASA's mission of understanding of the Cosmos by developing cost effective solutions that yield a leap in performance and science data. 'Maikalani' in Hawaiian translates to, "knowledge we gain from the cosmos." Missions like Hubble have fundamentally changed humanity's view of the cosmos. Last year's Nobel prize in physics was a result of astronomical discoveries. $9B class JWST size (6.5 meter diameter) space telescopes, when launched are anticipated to rewrite our knowledge of physics. Here we report on a neoteric meta-material telescope mirror technology designed to enable a factor of 100 or more reduction in areal density, a factor of 100 reduction in telescope production and launch costs as well as other advantages; a leap to enable missions to image the cosmos in unprecedented detail, with the associated gain in knowledge. Whether terahertz, visible or X-ray, reflectors used for high quality electromagnetic imaging require shape accuracy (surface figure) to far better than 1 wavelength (lambda) of the incident photons, more typically lambda/10 or better. Imaging visible light therefore requires mirror surfaces that approximate a desired curve (e.g. a sphere or paraboloid) with smooth shape deviation of th less than approximately 1/1000 the diameter of a human hair. This requires either thick high modulus material like glass or metal, or actuators to control mirror shape. During Phase I our team studied a novel solution to this systems level design mass/shape tradespace requirement both to advance the innovative space technology concept and also to help NASA and other agencies meet current operational and future mission requirements. Extreme and revolutionary NASA imaging missions such as Terrestrial Planet Imager (TPI) require lightweight mirrors with minimum diameters of 20 to 40 meters. For reference, NASA's great achievement; the Hubble space telescope, is only 2.4 meters in diameter. What is required is a way to make large inexpensive deployable mirrors where the cost is measured in millions, not billions like current efforts. For example we seek an interim goal within 10 years of a Hubble size (2.4m) primary mirror weighing 1 pound at a cost of 10K in materials. Described here is a technology using thin ultra lightweight materials where shape can be controlled simply with a beam of light, allowing imaging with incredibly low mass yet precisely shaped mirrors. These " Photonic Muscle" substrates will eventually make precision control of giant s p a c e apertures (mirrors) possible. OCCAM substrates make precision control of giant ultra light-weight mirror apertures possible. This technology is posed to create a revolution in remote sensing by making large ultra lightweight space telescopes a fiscal and material reality over the next decade.

Cosmos↗

Detalied X-ray observations of the Cygnus Loop

High quality X-ray spectra and imaging observations of the Cygnus Loop have been obtained with three different instruments. The High Resolution Imager (HRI) on the Einstein Observatory was used to obtain arcsecond resolution images of select bright regions in the Cygnus Loop which permit detailed comparisons between the X-ray, optical, and radio structure of the Loop. The Imaging Proportional Counter (IPC) on the Einstein Observatory was used to obtain an arcminute resolution map of essentially the full Loop structure. Finally, an Imaging Gas Scintillation Proportional Counter (IGSPC), carried aloft by a sounding rocket last fall, obtained modest resolution, spatially resolved spectrophotometry of the Cygnus Loop. An X-ray map of the Loop in the energy of the O VIII line was obtained. These data combine to yield a very powerful probe of the abundance, temperature, and density distribution of material in the supernova remnant, and in the interstellar medium.

Ku, W. H.-M.↗

Rapid Prototyping Integrated With Nondestructive Evaluation and Finite Element Analysis

Most reverse engineering approaches involve imaging or digitizing an object then creating a computerized reconstruction that can be integrated, in three dimensions, into a particular design environment. Rapid prototyping (RP) refers to the practical ability to build high-quality physical prototypes directly from computer aided design (CAD) files. Using rapid prototyping, full-scale models or patterns can be built using a variety of materials in a fraction of the time required by more traditional prototyping techniques (refs. 1 and 2). Many software packages have been developed and are being designed to tackle the reverse engineering and rapid prototyping issues just mentioned. For example, image processing and three-dimensional reconstruction visualization software such as Velocity2 (ref. 3) are being used to carry out the construction process of three-dimensional volume models and the subsequent generation of a stereolithography file that is suitable for CAD applications. Producing three-dimensional models of objects from computed tomography (CT) scans is becoming a valuable nondestructive evaluation methodology (ref. 4). Real components can be rendered and subjected to temperature and stress tests using structural engineering software codes. For this to be achieved, accurate high-resolution images have to be obtained via CT scans and then processed, converted into a traditional file format, and translated into finite element models. Prototyping a three-dimensional volume of a composite structure by reading in a series of two-dimensional images generated via CT and by using and integrating commercial software (e.g. Velocity2, MSC/PATRAN (ref. 5), and Hypermesh (ref. 6)) is being applied successfully at the NASA Glenn Research Center. The building process from structural modeling to the analysis level is outlined in reference 7. Subsequently, a stress analysis of a composite cooling panel under combined thermomechanical loading conditions was performed to validate this process.

Abdul-Aziz, Ali↗

Fluorescent Applications to Crystallization

By covalently modifying a subpopulation, less than or equal to 1%, of a macromolecule with a fluorescent probe, the labeled material will add to a growing crystal as a microheterogeneous growth unit. Labeling procedures can be readily incorporated into the final stages of purification, and tests with model proteins have shown that labeling u to 5 percent of the protein molecules does not affect the X-ray data quality obtained . The presence of the trace fluorescent label gives a number of advantages. Since the label is covalently attached to the protein molecules, it "tracks" the protein s response to the crystallization conditions. The covalently attached probe will concentrate in the crystal relative to the solution, and under fluorescent illumination crystals show up as bright objects against a darker background. Non-protein structures, such as salt crystals, do not show up under fluorescent illumination. Crystals have the highest protein concentration and are readily observed against less bright precipitated phases, which under white light illumination may obscure the crystals. Automated image analysis to find crystals should be greatly facilitated, without having to first define crystallization drop boundaries as the protein or protein structures is all that shows up. Fluorescence intensity is a faster search parameter, whether visually or by automated methods, than looking for crystalline features. Preliminary tests, using model proteins, indicates that we can use high fluorescence intensity regions, in the absence of clear crystalline features or "hits", as a means for determining potential lead conditions. A working hypothesis is that more rapid amorphous precipitation kinetics may overwhelm and trap more slowly formed ordered assemblies, which subsequently show up as regions of brighter fluorescence intensity. Experiments are now being carried out to test this approach using a wider range, of proteins. The trace fluorescently labeled crystals will also emit with sufficient intensity to aid in the automation of crystal alignment using relatively low cost optics, further increasing throughput at synchrotrons.

Pusey, Marc L.↗

Martian Polar Region Impact Craters: Topographical Perspectives from the Mars Orbiter Laser Altimeter

The Mars Orbiter Laser Altimeter (MOLA) has acquired over 100 topographic cross-sections of impact landforms in the polar regions of Mars as part of Mars Global Surveyor (MGS) Science Phasing Orbit observations during the period from April to July, 1998. These MOLA topographic profiles offer the first three-dimensional perspectives of high latitude craters on Mars yet available, and provide evidence of landform geometries not previously recognized. Indeed, the relatively poor quality of Viking Orbiter images of many high northern latitude regions has allowed the MOLA data to provide insights into the cavities and ejecta topologies of non-degraded impact landforms that have clearly experienced interactions with condensates, either as part of their formation, or as a post-modification stage effect. Here we report a preliminary summary of the results associated with topographic measurements for a statistically significant population of impact features all of which lie north of 60N latitude. MOLA sampled four impact features with frost-related interior deposits, including the 81 km (diameter) Korolev feature. In several cases, there is evidence from near-centerline MOLA cross-sections of crater interior features (i.e., central peak or ice-dust deposits) that are anomalously large relative to the crater cavity. Central structures that make up more than 50% of the volume of a crater cavity are observed, suggesting that either substantial accumulation of mantling materials has occurred, or that crater excavation triggered production of volume-enhancing materials (ice?). Pedestal craters sampled by MOLA also attest to enhanced production of ejecta materials in high latitude terrains. For example, many of the pedestal craters suggest a volume of ejecta (Ve) to volume of cavity (Vc) ratio far in excess of 1.0 (i.e., over 3.0), even in cases where the floor of the cavity appears unfilled. Finally, the well-defined transitions between simple and complex craters observed in MOLA data for non-polar latitude impact features is not preserved at high northern latitudes (for non-degraded craters). This further suggests the role of target materials (i.e., frozen volatiles?) in the cratering process on Mars in such regions.

Garvin, J. B.↗

Crystal Growth of II-VI Semiconducting Alloys by Directional Solidification

This research study is investigating the effects of a microgravity environment during the crystal growth of selected II-VI semiconducting alloys on their compositional, metallurgical, electrical and optical properties. The on-going work includes both Bridgman-Stockbarger and solvent growth methods, as well as growth in a magnetic field. The materials investigated are II-VI, Hg(1-x)Zn(x)Te, and Hg(1-x)Zn(x)Se, where x is between 0 and 1 inclusive, with particular emphasis on x-values appropriate for infrared detection and imaging in the 5 to 30 micron wavelength region. Wide separation between the liquidus and solidus of the phase diagrams with consequent segregation during solidification and problems associated with the high volatility of one of the components (Hg), make the preparation of homogeneous, high-quality, bulk crystals of the alloys an extremely difficult nearly an impossible task in a gravitational environment. The three-fold objectives of the on-going investigation are as follows: (1) To determine the relative contributions of gravitationally-driven fluid flows to the compositional redistribution observed during the unidirectional crystal growth of selected semiconducting solid solution alloys having large separation between the liquidus and solidus of the constitutional phase diagram; (2) To ascertain the potential role of irregular fluid flows and hydrostatic pressure effects in generation of extended crystal defects and second-phase inclusions in the crystals; and, (3) To obtain a limited amount of "high quality" materials needed for bulk crystal property characterizations and for the fabrication of various device structures needed to establish ultimate material performance limits. The flight portion of the study was to be accomplished by performing growth experiments using the Crystal Growth Furnace (CGF) manifested to fly on various Spacelab missions.

Lehoczky, Sandor L.↗

Real-Time X-ray Radiography Diagnostics of Components in Solid Rocket Motors

Solid rocket motors (SRMs) typically use nozzle materials which are required to maintain their shape as well as insulate the underlying support structure during the motor operation. In addition, SRMs need internal insulation materials to protect the motor case from the harsh environment resulting from the combustion of solid propellant. In the nozzle, typical materials consist of high density graphite, carbon-carbon composites and carbon phenolic composites. Internal insulation of the motor cases is typically a composite material with carbon, asbestos, Kevlar, or silica fibers in an ablative matrix such as EPDM or NBR. For both nozzle and internal insulation materials, the charring process occurs when the hot combustion products heat the material intensely. The pyrolysis of the matrix material takes away a portion of the thermal energy near the wall surface and leaves behind a char layer. The fiber reinforcement retains the porous char layer which provides continued thermal protection from the hot combustion products. It is of great interest to characterize both the total erosion rates of the material and the char layer thickness. By better understanding of the erosion process for a particular ablative material in a specific flow environment, the required insulation material thickness can be properly selected. The recession rates of internal insulation and nozzle materials of SRMs are typically determined by testing in some sort of simulated environment; either arc-jet testing, flame torch testing, or subscale SRMs of different size. Material recession rates are deduced by comparison of pre- and post-test measurements and then averaging over the duration of the test. However, these averaging techniques cannot be used to determine the instantaneous recession rates of the material. Knowledge of the variation in recession rates in response to the instantaneous flow conditions during the motor operation is of great importance. For example, in many SRM configurations the recession of the solid propellant grain can drastically alter the flow-field and effect the recession of internal insulation and nozzle materials. Simultaneous measurement of the overall erosion rate, the development of the char layer, and the recession of the char-virgin interface during the motor operation can be rather difficult. While invasive techniques have been used with limited success, they have serious drawbacks. Break wires or make wire sensors can be installed into a sufficient number of locations in the charring material from which a time history of the charring surface can be deduced. These sensors fundamentally alter the local structure of the material in which they are imbedded. Also, the location of these sensors within the material is not known precisely without the use of an X-ray. To determine instantaneous recession rates, real-time X-ray radiography (X-ray RTR) has been utilized in several SRM experiments at PSU. The X-ray RTR system discussed in this paper consists of an X-ray source, X-ray image intensifier, and CCD camera connected to a capture computer. The system has been used to examine the ablation process of internal insulation as well as nozzle material erosion in a subscale SRM. The X-ray source is rated to 320 kV at 10 mA and has both a large (5.5 mm) and small (3.0 mm) focal spot. The lead-lined cesium iodide X-ray image intensifier produces an image which is captured by a CCD camera with a 1,000 x 1,000 pixel resolution. To produce accurate imagery of the object of interest, the alignment of the X-ray source to the X-ray image intensifier is crucial. The image sequences captured during the operation of an SRM are then processed to enhance the quality of the images. This procedure allows for computer software to extract data on the total erosion rate and the char layer thickness. Figure 1 Error! Reference source not found.shows a sequence of images captured during the operation the subscale SRM with the X-ray RTR system. The X-rayTR system, alignment procedure, uncertainty determination, and image analysis process will be discussed in detail in the full manuscript.

Cortopassi, A. C.↗

Fluorescent Approaches to High Throughput Crystallography

X-ray crystallography remains the primary method for determining the structure of macromolecules. The first requirement is to have crystals, and obtaining them is often the rate-limiting step. The numbers of crystallization trials that are set up for any one protein for structural genomics, and the rate at which they are being set up, now overwhelm the ability for strictly human analysis of the results. Automated analysis methods are now being implemented with varying degrees of success, but these typically cannot reliably extract intermediate results. By covalently modifying a subpopulation, less than or = 1 %, of a macromolecule solution with a fluorescent probe, the labeled material will add to a growing crystal as a microheterogeneous growth unit. Labeling procedures can be readily incorporated into the final stages of purification. The covalently attached probe will concentrate in the crystal relative to the solution, and under fluorescent illumination the crystals show up as bright objects against a dark background. As crystalline packing is more dense than amorphous precipitate, the fluorescence intensity can be used as a guide in distinguishing different types of precipitated phases, even in the absence of obvious crystalline features, widening the available potential lead conditions in the absence of clear "hits." Non-protein structures, such as salt crystals, will not incorporate the probe and will not show up under fluorescent illumination. Also, brightly fluorescent crystals are readily found against less fluorescent precipitated phases, which under white light illumination may serve to obscure the crystals. Automated image analysis to find crystals should be greatly facilitated, without having to first define crystallization drop boundaries and by having the protein or protein structures all that show up. The trace fluorescently labeled crystals will also emit with sufficient intensity to aid in the automation of crystal alignment using relatively low cost optics, further increasing throughput at synchrotrons. Preliminary experiments show that the presence of the fluorescent probe does not affect the nucleation process or the quality of the X-ray data obtained.

Pusey, Marc L.↗